CN101918814A - Method for operating an FTIR spectrometer, and FTIR spectrometer - Google Patents

Method for operating an FTIR spectrometer, and FTIR spectrometer Download PDF

Info

Publication number
CN101918814A
CN101918814A CN2008801170089A CN200880117008A CN101918814A CN 101918814 A CN101918814 A CN 101918814A CN 2008801170089 A CN2008801170089 A CN 2008801170089A CN 200880117008 A CN200880117008 A CN 200880117008A CN 101918814 A CN101918814 A CN 101918814A
Authority
CN
China
Prior art keywords
gas
spectrometer
calibration
checking
place
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN2008801170089A
Other languages
Chinese (zh)
Inventor
N·威尔
B·希尔舍
C·贝克尔
B·安德列斯
C·拉特克
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
ABB AB
Original Assignee
Asea Brown Boveri AB
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Asea Brown Boveri AB filed Critical Asea Brown Boveri AB
Publication of CN101918814A publication Critical patent/CN101918814A/en
Pending legal-status Critical Current

Links

Images

Classifications

    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/27—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands using photo-electric detection ; circuits for computing concentration
    • G01N21/274—Calibration, base line adjustment, drift correction
    • G01N21/276—Calibration, base line adjustment, drift correction with alternation of sample and standard in optical path
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/01—Arrangements or apparatus for facilitating the optical investigation
    • G01N21/13—Moving of cuvettes or solid samples to or from the investigating station
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/27—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands using photo-electric detection ; circuits for computing concentration
    • G01N21/274—Calibration, base line adjustment, drift correction
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
    • G01N21/3504—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing gases, e.g. multi-gas analysis
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01J—MEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
    • G01J3/00—Spectrometry; Spectrophotometry; Monochromators; Measuring colours
    • G01J3/28—Investigating the spectrum
    • G01J2003/2866—Markers; Calibrating of scan
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01J—MEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
    • G01J3/00—Spectrometry; Spectrophotometry; Monochromators; Measuring colours
    • G01J3/28—Investigating the spectrum
    • G01J2003/2866—Markers; Calibrating of scan
    • G01J2003/2879—Calibrating scan, e.g. Fabry Perot interferometer
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01J—MEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
    • G01J3/00—Spectrometry; Spectrophotometry; Monochromators; Measuring colours
    • G01J3/28—Investigating the spectrum
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01J—MEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
    • G01J3/00—Spectrometry; Spectrophotometry; Monochromators; Measuring colours
    • G01J3/28—Investigating the spectrum
    • G01J3/42—Absorption spectrometry; Double beam spectrometry; Flicker spectrometry; Reflection spectrometry
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/01—Arrangements or apparatus for facilitating the optical investigation
    • G01N21/03—Cuvette constructions
    • G01N2021/0357—Sets of cuvettes
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/01—Arrangements or apparatus for facilitating the optical investigation
    • G01N21/03—Cuvette constructions
    • G01N2021/0367—Supports of cells, e.g. pivotable
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N2021/3196—Correlating located peaks in spectrum with reference data, e.g. fingerprint data
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
    • G01N2021/3595—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light using FTIR
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/01—Arrangements or apparatus for facilitating the optical investigation
    • G01N21/03—Cuvette constructions
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/01—Arrangements or apparatus for facilitating the optical investigation
    • G01N21/03—Cuvette constructions
    • G01N21/05—Flow-through cuvettes
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/0004—Gaseous mixtures, e.g. polluted air
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/0004—Gaseous mixtures, e.g. polluted air
    • G01N33/0006—Calibrating gas analysers

Abstract

The invention relates to a method for operating a FTIR (Fourier transformation infrared) spectrometer, wherein a validation/calibration of the spectrometer is carried out in cyclically recurring intervals in that by way of at least two temporarily available gases a reference spectrum with a zero gas and also an absorption spectrum with a calibration gas are recorded. The invention further relates to a spectrometer according to the preamble of the patent claims 1 and 8. In order to achieve that at each site of use and at any time a calibration or validation of the spectrometer can be carried out, the invention proposes to use so-called substitute gases during the validation of the spectrometer as gas components, said substitute gases only simulating the actual measured gas component with respect to the metrological properties.

Description

The method of operating of FTIR spectrometer and FTIR spectrometer
Technical field
The present invention relates to method of operating and FTIR spectrometer itself according to FTIR (Fourier transform infrared) spectrometer of claim 1 and 8 preambles.
Background technology
The FTIR spectrometer is the infrared spectrometer with the computing method work of Fourier transform.This spectrometer is not based on the work of specific absorption spectral line, but writes down the spectrum of whole wavelength coverage and obtain information about the absorption on observed frequency spectrum or the wavelength spectrum (Wellenlaengenspektrum) by means of the spectrometer function (Spektrometerfunktion) of mathematics thus.Carry out stoichiometry (chemometrisch) analysis according to the distribution that is obtained then, and corresponding gas componant is distributed in distribution.Therefore, can measure a plurality of gas componants simultaneously with the FTIR spectrometer.
For by above-mentioned all frequency ranges, use to have the movably interferometer structure work of mirror, for example Michelson (Michelson) interferometer structure.
For device-dependent (geraetebedingt) drift that the change of for example eliminating by transport property causes, must periodic calibration and checking.Only in this way just can guarantee the reliability of measurement result.For easy-to-handle gas componant, such as CO or CO 2, this may be simple.But in general, the FTIR spectrometer also is interested for reluctant gas.This comprises for example NH 3, HCI, HF, H 2O.
But the advantage of FTIR spectrometer is to measure a plurality of gas componants simultaneously.Therefore, this spectrometer especially also is suitable for emission measurement (Emissonsmessung).Usually carry out the inspection of spectrometer every day.
The inspection of calibration data (checking) is carried out with two steps at present usually: the periodic logging that carries out baseline spectrum with short interval (normally every day) with zero gas (Nullgas) (outside air after normally purifying).Come the variation of the transport property of bucking-out system with this baseline spectrum.The variation of transport property for example can be caused by the variation of the variation of the pollution in the optical path, radiation power, detector or by the contamination of measuring unit.The compensation at zero point depends on that wavelength ground carries out, and therefore proofreaies and correct for all constituents at zero point simultaneously.
Is that all constituents carries out the regular checking (inspection) of reference point and also calibrates under possible situation with longer interval (normally jede Woche to annual) with test gas.Easy to handle gas, such as CO, CO 2, NO can be calibrated with the test gas in the test gas bottle under the situation of not additional aid.For the composition that is difficult in the test gas bottle, handle, such as H 2O or HCI, the service test gas generator replaces the test gas bottle.But such processing is difficulty very, and almost can not carry out in some places to use of spectrometer.
The checking of reference point or calibration may be performed under the high situation of technology and time cost, especially when such as H 2When the such gas of O or HCI must be calibrated.Its reason for example is:
-additional technical equipment is installed, such as the test gas generator
-for HCI and H 2The adjusting time that O is long
The calibration that the wrong concentration of-carburetor may lead to errors.
Therefore the checking of reference point and/or calibration can only be undertaken by trained expert.
Therefore, reference point only is examined with the long time interval, does not promptly have the checking of reference point at interval for long measurement.This causes the mistake of concentration to show that risk increases.
US 5,777,735 disclose so a kind of method and apparatus, wherein as other known methods, at gas componant to be measured separately equipment is calibrated in the following manner, promptly the corresponding gas of respective pure form is presented from hold the air-capacitor device as calibration gas.For majority of gas, this is too expensive.
Summary of the invention
Therefore, technical matters to be solved by this invention is further to improve such method and spectrometer, makes in any place to use, can carry out the calibration and the checking of spectrometer at any time.
According to the present invention, for such method, this technical matters is to solve by the feature in claim 1 characteristic.
Other preferred implementations of the method according to this invention provide in dependent claims 2 to 7.
For such spectrometer, according to the present invention, this technical matters is to solve by the feature in claim 8 characteristic.
Other favourable embodiments provide in all the other dependent claims.
The core of the present invention aspect method be, when the checking spectrometer, as to the additional of actual measurement composition or substitute, can also select to cover the easy to handle place of gas composition of the whole spectral limit of spectrometer.For measuring such as HCI, HF, NH 3Reluctant other application scenarios like this, advantageously: can avoid following situation with the method according to this invention, promptly for effectively checking or calibration, above-mentioned gas must be provided with high-purity as test gas.In contrast, use easy-to-handle gas to be used for checking as an alternative, these easy-to-handle gases roughly produce absorption effect in the scope of " difficulty " gas, almost as representative.Thereby, if actual measurement gas for calibrate must with highly purified form and accurately concentration provide, compare with actual measurement gas as checking or this place of gas of calibration gas and be easier to significantly handle.Wherein in the following place of gas that is called as, place of gas obviously is not to be aggressive (aggresiv) or be difficult to like that handle as those gases that it should be represented.Whole checking and calibration become simpler thus.
In another favourable embodiment, the mixed gas that is made of a plurality of place of gas is used to checking, and these a plurality of place of gas cover the sub-range of whole measurement spectrum respectively.By this way, the place of gas that is used for calibrating can be introduced into mixed gas, and this has been chemically adventurous with the actual gas composition.In this way, can in a step, verify the complete spectrum scope of spectrometer immediately.
In another favourable embodiment, so a plurality of place of gas are introduced in the calibration/verification mixed gas, make these place of gas cover the whole spectral limit of spectrometer.
In another favourable embodiment, also monitor the intensity in the checking/calibration steps that uses zero gas, thereby and pass through interpolation and store whole spectrum as benchmark.
In another favourable embodiment, place of gas separately, promptly hold the air-capacitor device from difference, perhaps mixed gas holds the air-capacitor device by single valve control device (Einzelventilansteuerung) from one and is automatically presenting to measuring vessel (Messkuevette) in the checking/calibration steps automatically as an alternative, carries out then and verifies accordingly or calibration steps.Therefore, carry out verification step with the simple and effective way Automatic Cycle.
In another favourable embodiment, determined checking or calibration value are stored in the self-adapting data district, wherein can be as required according to this Data Base Analysis checking/calibration history, so that therefrom obtain the diagnosis of the maintenance state of relevant spectrometer where necessary.
In the end in favourable embodiment, place of gas separately or as an alternative mixed gas is closed, promptly is enclosed in the calibrated vessel (Kalibrierkuevette) and in order to carry out checking/calibration steps, this calibrated vessel changes in (einschwenken) light path automatically, produces from light path again then.
For the FTIR spectrometer, core of the present invention is: such gas is used as the calibration means, promptly this gas only is the representative of actual measurement gas with regard to the assimilation effect in the spectrometer with regard to it, and be stored in and hold in the air-capacitor device, and can automated serial ground when automatically starting calibration or proof procedure one by one or be incorporated into as mixed gas in the light path of spectrometer.
In the favourable embodiment according to spectrometer of the present invention, gas can be introduced in the measuring vessel of spectrometer by means of the automatic valve control device.Therefore, calibration process can be started automatically, and gas is introduced into.
In an alternate embodiments, gas can and can produce again after calibration/verification in the one or more light paths that change spectrometer in gas is filled the calibrated vessel of rear enclosed automatically over to automatically.Therefore, no longer need gas storage.
Description of drawings
Structure at the method according to this invention and spectrometer shows the present invention in the accompanying drawings, and following detailed description the present invention.
In the accompanying drawing:
Fig. 1 shows the principle structure with FTIR spectrometer rotatable or movably calibrated vessel.
Fig. 2 shows the control of calibration.
Fig. 3 shows the spectrum with guide's composition (Leitkomponent) (representative).
Fig. 4 shows the division of spectrum in the zone.
Embodiment
Fig. 1 illustrates the principle structure of FTIR spectrometer, and it for example is arranged on the Michelson interferometer.From radiation source 5, generate parallel light beam by means of first optical system 4 by expansion (Aufweitung), parallel light beam is fallen the semitransparent mirror 3 as beam splitting equipment.Have fixed wave length and the frequency location (monochromatic with relevant) of light drop on now on the fixing mirror 1 and also are reflected there.Other beamlets pass mirror 3 as the crow flies, and by the direction of mirror 2 reflected back mirrors 3 movably, these two beamlets interfere with each other at Jing3Chu now.This interference at this by controllably being handled along optical axis moving lens 2.Begin therefrom, interference light transmission measurement container 8, wherein measurement gas is directed by this measuring vessel.By means of interferometer, measuring vessel, and point-device adjusting of effective frequency position of therefore hitting the light beam of measurement gas have been realized hitting.Therefore, can gather complete spectrum at the detecting device place, and the absorptivity when being not only fixed frequency.For irradiating and detecting device optimally, the light beam of expansion is focused again by second optical system 6, promptly focuses on the yardstick of detecting device.
Measuring vessel air inclusion inlet A and gas vent B, and be introduced into to write down with measurement gas and measure spectrum, again it is drawn then.
In order to carry out according to calibration steps of the present invention, being controlled at this does not now have the valve control device that further shows, and calibration gas is directed or blows and dash by container 8, so that the measurement gas that will measure by valve commutation introducing after calibration.
In another alternative this illustrate, wherein the duration of calibration or checking, calibration gas is being changed in the light path before the detecting device 7 or before optical system 6 by means of calibrated vessel 9.Then, calibrated vessel produces from light path again.
Wherein important will point out, calibrated vessel is not filled being calibrated measured measurement of correlation gas or measurement gas composition in the part at this of spectrometer, but is filled place of gas or alternative mixed gas to represent this measurement of correlation gas or these measurement gas compositions.Therefore, on the spectral limit of spectrometer, for example use SO 2, CO 2, N 2O or methane is gas as an alternative, promptly as representative, rather than very thorny gas componant HCI, HF, NH 3Deng.It is obviously more expensive that the latter is used to calibrate with respective pure form.On the contrary, the place of gas of replacement used according to the invention has just been simplified calibration/verification significantly, because these described alternative compositions can obviously more easily be handled.They are handled so easily, to such an extent as to they are not to calibrate in gas delivery method, now also can handle in airtight calibrated vessel.This is in the past with HCI or HF or even use water vapor H 2O is impossible.
When using calibrated vessel, each gas can be enclosed in the calibrated vessel equally respectively, and can alternately change over to a kind of chopper of form, perhaps the mixed gas of a plurality of place of gas in the gas delivery method, using a common calibration container 9.
Replace changing motion over to, calibrated vessel also can change over to rectilinear motion certainly.
Fig. 2 shows the control according to FTIR of the present invention on principle.Wherein, carry out the manipulation of light source 5 (laser instrument) and detecting device 7 by control module 10.Time control unit 11 triggers calibration process in adjustable time or by clear and definite control signal.For this reason, control mirror 2, light source 5 and detecting device 7 now in phase, and control changing over to or moving and handle of calibrated vessel 9 for this reason in phase, and therefore baseline spectrum is recorded and is stored in the self-adaptation storage unit 12.In addition, storage unit 12 also have the time distributively record data additionally can discern possible aging effect Analysis thus as historical data.Thus, except pure calibration, also carry out the lasting self diagnosis of spectrometer.
Replace changing over to or moving of control calibrated vessel, also can be controlled at the valve control device that is used to present place of gas in the carrying method in phase, so that by using above-mentioned place of gas also to carry out calibration in this mode.
Fig. 3 shows, and replaces the test gas task for all the components, how to verify (inspection) by the test mixed gas that is made of a plurality of place of gas.Place of gas can all be mixed together in the test gas bottle, and stable on a long time interval.Place of gas also can be to measure composition, for example SO 2Or CO 2But, alternatively or additionally, also can use the gas that in different wavelength range, has a plurality of absorptions, for example stable halogenated hydrocarbon or N 2O and CO 2Ideally, place of gas covers the whole spectral limit of spectrometer.
For example, can use following place of gas for this reason.
-long-wave limit is for example used SO 2
-intermediate range is for example used CO 2
-shortwave scope is by methane and N 2O
How additionally Fig. 4 shows the intensity of monitoring criteria spectrum.Therefore, also monitor the wavelength coverage that not replaced gas covers.
If when the checking spectrometer, do not occur the variation of place of gas or each scope of baseline spectrum now, the variation at zero point does not appear, and then do not exist residue to measure the variation of composition (for example HCI or HF) yet.
Opposite with the checking/calibration of service test gas generator, the end of whole process can be by robotization.That is, be used for the zero gas of baseline spectrum and place of gas the test mixed gas can by solenoid valve such computer control as described be stopped.The result can be analyzed automatically, and can trigger warning where necessary.Under than the situation of low deviation, also can trigger warning.
Storage to the checking outcome history can be used as the basis that is used for the continuous mass monitoring.In addition, can store the spectrum of guide's composition and reference value, as previously mentioned.
Alternatively, also can not use the test gas bottle with place of gas constituents mixt fully, method is: be enclosed in the calibrated vessel to the place of gas stable components.Replace test gas task, so calibrated vessel changes in the optical path as mentioned above circularly by solenoid valve.
Reference numerals list
1. the mirror of fixing
2. mirror movably
3. translucent mirror/beam beam splitting equipment
4. the optical system of expanding
5. radiation source
6. the optical system that focuses on
7. detecting device
8. measuring vessel
9. calibrated vessel
10. control device
11. time-controlling arrangement
12. self-adapting data storer
A measurement gas inlet
The outlet of B measurement gas

Claims (10)

  1. The method of operating of (1.FTIR fourier-transform infrared) spectrometer, wherein at least two gases that temporarily provide had both write down the baseline spectrum of use zero gas, also record uses the absorption spectra of calibration gas by using, carry out the checking/calibration of described spectrometer with the interval that circulation repeats, it is characterized in that, when the checking spectrometer, use so-called place of gas as gas componant, the measurement gas composition of wherein said place of gas only simulation reality with regard to the measuring technique characteristic.
  2. 2. method according to claim 1 is characterized in that, the mixed gas that is made of a plurality of place of gas is used to checking, and wherein said place of gas covers the subregion of whole measurement spectrum respectively.
  3. 3. method according to claim 2 is characterized in that, introduces so a plurality of place of gas in introducing the calibration/verification mixed gas, makes these place of gas cover the whole spectral limit of spectrometer.
  4. 4. according to each described method in the aforementioned claim, it is characterized in that also the intensity of baseline spectrum in the checking/calibration steps of zero gas is used in monitoring, thereby and by interpolation, whole spectrum is stored as benchmark.
  5. 5. according to each described method in the aforementioned claim, it is characterized in that, described place of gas separately, promptly hold the air-capacitor device from difference, perhaps hold the air-capacitor device from one and automatically presenting to measuring vessel in the checking/calibration steps automatically, carry out corresponding checking or calibration steps then by single valve control device as mixed gas.
  6. 6. method according to claim 5, it is characterized in that, determined checking or calibration value are stored in the self-adapting data district, wherein can be as required according to this Data Base Analysis checking/calibration history, so that therefrom obtain the diagnosis of the maintenance state of relevant spectrometer where necessary.
  7. 7. according to each described method in the aforementioned claim, it is characterized in that, described place of gas separately or as an alternative mixed gas is closed, promptly is enclosed in the calibrated vessel, and in order to carry out checking/calibration steps, this calibrated vessel changes in the light path automatically, produces from light path again then.
  8. 8. the FTIR spectrometer that has checking and/or calibrating installation, be used for verifying circularly and/or calibrating the measurement spectrum of FTIR spectrometer, it is characterized in that, such gas is used as the calibration means, promptly this gas only is the representative of actual measurement gas with regard to the assimilation effect in the spectrometer with regard to it, and be stored in and hold in the air-capacitor device, and can automated serial ground when automatically starting calibration or proof procedure one by one or be incorporated into as mixed gas in the light path of spectrometer.
  9. 9. FTIR spectrometer according to claim 8 is characterized in that, described gas can be introduced in the measuring vessel of spectrometer by means of the automatic valve control device.
  10. 10. FTIR spectrometer according to claim 8 is characterized in that, described gas can and can produce again after calibration/verification in the one or more light paths that change spectrometer in gas is filled the calibrated vessel of rear enclosed automatically over to automatically.
CN2008801170089A 2007-11-22 2008-11-21 Method for operating an FTIR spectrometer, and FTIR spectrometer Pending CN101918814A (en)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE102007056345A DE102007056345B3 (en) 2007-11-22 2007-11-22 Method for operating fourier transformation infrared-spectrometer, involves utilizing residual gases as gas components in each case during validation of spectrometer, which simulate actual measuring gas component
DE102007056345.2 2007-11-22
PCT/EP2008/009854 WO2009065595A1 (en) 2007-11-22 2008-11-21 Method for operating an ftir spectrometer, and ftir spectrometer

Publications (1)

Publication Number Publication Date
CN101918814A true CN101918814A (en) 2010-12-15

Family

ID=40076286

Family Applications (1)

Application Number Title Priority Date Filing Date
CN2008801170089A Pending CN101918814A (en) 2007-11-22 2008-11-21 Method for operating an FTIR spectrometer, and FTIR spectrometer

Country Status (5)

Country Link
US (1) US20100282958A1 (en)
EP (1) EP2215454A1 (en)
CN (1) CN101918814A (en)
DE (1) DE102007056345B3 (en)
WO (1) WO2009065595A1 (en)

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103403529A (en) * 2010-12-23 2013-11-20 Abb股份公司 Optical gas analyser device having means for calibrating the frequency spectrum
CN103635785A (en) * 2011-02-15 2014-03-12 勒克思马克斯科技公司 A fully integrated complementary metal oxide semiconductor (CMOS) fourier transform infrared (FTIR) spectrometer and raman spectrometer and method thereof
CN108072624A (en) * 2016-11-18 2018-05-25 天津邦纳科技有限公司 A kind of method that amount of nitrogen oxides chemical sensor and spectrometer mutually verify
CN108072623A (en) * 2016-11-18 2018-05-25 天津邦纳科技有限公司 A kind of method that content of sulfur dioxide chemical sensor and spectrometer mutually verify
CN112540053A (en) * 2020-09-27 2021-03-23 杭州春来科技有限公司 Open type gas detection device

Families Citing this family (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2635902B1 (en) * 2010-11-01 2018-12-12 Koninklijke Philips N.V. A method of calibrating an air sensor
US8467996B2 (en) 2011-02-09 2013-06-18 Jorge E Perez Spectral analysis operating system
RU2571185C2 (en) * 2011-08-19 2015-12-20 ФОСС Аналитикал А/С Method to compensate for amplitude drift in spectrometer and spectrometer realising specified method
DE102013101610B4 (en) * 2013-02-19 2015-10-01 Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. Apparatus and method for remote detection of a non-infrared active target gas
DE102013005997B3 (en) * 2013-04-08 2014-05-15 Abb Technology Ag Optical gas analyzer device for use with industrial chimney of waste-incineration plant, has processing unit determining gas concentration of total carbon contained in measurement gas other than analyzing pollutant components
US20230014558A1 (en) * 2021-07-06 2023-01-19 Si-Ware Systems Self-calibrated spectroscopic and ai-based gas analyzer

Family Cites Families (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE4128912C2 (en) * 1991-08-30 1995-06-22 Deutsche Forsch Luft Raumfahrt Method and device for the calibration of spectroradiometers
US5777735A (en) * 1996-09-30 1998-07-07 Minnesota Mining And Manufacturing Company In situ analysis apparatus
CA2267558C (en) * 1998-04-10 2005-09-13 Her Majesty The Queen, In Right Of Canada, As Represented By The Ministe R Of National Defence Fourier-transform spectrometer configuration optimized for self emission suppression and simplified radiometric calibration
US7535006B2 (en) * 2003-06-09 2009-05-19 Canberra Albuquerque, Inc. Gaseous uranium hexafluride isotope measurement by diode laser spectroscopy
JP4591105B2 (en) * 2004-05-31 2010-12-01 横河電機株式会社 Calibration method
DE102004031643A1 (en) * 2004-06-30 2006-02-02 Abb Patent Gmbh Non-dispersive infrared gas analyzer
US7598494B2 (en) * 2007-01-30 2009-10-06 Airgas, Inc. Automated FTIR gas analyzer

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103403529A (en) * 2010-12-23 2013-11-20 Abb股份公司 Optical gas analyser device having means for calibrating the frequency spectrum
CN103403529B (en) * 2010-12-23 2015-07-22 Abb股份公司 Optical gas analyser device having means for calibrating the frequency spectrum
CN103635785A (en) * 2011-02-15 2014-03-12 勒克思马克斯科技公司 A fully integrated complementary metal oxide semiconductor (CMOS) fourier transform infrared (FTIR) spectrometer and raman spectrometer and method thereof
CN103635785B (en) * 2011-02-15 2016-11-02 勒克思马克斯科技公司 Integrate CMOS-FTIR measures and Raman measures spectrogrph and method thereof
CN108072624A (en) * 2016-11-18 2018-05-25 天津邦纳科技有限公司 A kind of method that amount of nitrogen oxides chemical sensor and spectrometer mutually verify
CN108072623A (en) * 2016-11-18 2018-05-25 天津邦纳科技有限公司 A kind of method that content of sulfur dioxide chemical sensor and spectrometer mutually verify
CN112540053A (en) * 2020-09-27 2021-03-23 杭州春来科技有限公司 Open type gas detection device

Also Published As

Publication number Publication date
WO2009065595A1 (en) 2009-05-28
EP2215454A1 (en) 2010-08-11
DE102007056345B3 (en) 2009-01-02
US20100282958A1 (en) 2010-11-11

Similar Documents

Publication Publication Date Title
CN101918814A (en) Method for operating an FTIR spectrometer, and FTIR spectrometer
Workman A review of calibration transfer practices and instrument differences in spectroscopy
US10648840B2 (en) Spectrometer secondary reference calibration
Crosson A cavity ring-down analyzer for measuring atmospheric levels of methane, carbon dioxide, and water vapor
Chen et al. Accurate measurements of carbon monoxide in humid air using the cavity ring-down spectroscopy (CRDS) technique
CN101084419A (en) A method for standardising a spectrometer
Thoma et al. Open-path tunable diode laser absorption spectroscopy for acquisition of fugitive emission flux data
CN104903704B (en) Carry out the tunable diode laser absorption spectroscopy of steam measure
US9448215B2 (en) Optical gas analyzer device having means for calibrating the frequency spectrum
EP3133380A1 (en) Photodetector output correction method used for spectroscopic analyzer
CN103616338A (en) Reconstruction method for atmosphere trace gas spatial distribution by differential optical absorption spectroscopy tomoscan
JP6967387B2 (en) Gas analyzers, programs for gas analyzers, and gas analysis methods
JP2001153724A (en) Wavelength standard
US9638628B2 (en) Gas analysis system and method
Weibring et al. Multi-component chemical analysis of gas mixtures using a continuously tuneable lidar system
Briz et al. Remote sensing by open-path FTIR spectroscopy. Comparison of different analysis techniques applied to ozone and carbon monoxide detection
Di Paolantonio et al. A semi-automated procedure for the emitter-receiver geometry characterization of motor-controlled lidars
Guenard et al. Importance of prediction outlier diagnostics in determining a successful inter-vendor multivariate calibration model transfer
Rolle et al. Production and validation of primary carbon dioxide reference standards at INRIM
Dierks et al. Experimental Characterization of a Tuneable Diode Laser Absorption Spectroscopy Based Sensor
Kooijmans Carbonyl sulfide, a way to quantify photosynthesis
US20210333206A1 (en) Aerosol transmissometer with an in-process transfer standard
Ropertz et al. Calibration of a high-resolution open-path FTIR spectrometer combined with an adjustable 100-m multipass cell
Igne et al. 17 Calibration Transfer
Gaynullin et al. Implementation of NDIR technology for selective sensing of gases with common absorption spectra

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C12 Rejection of a patent application after its publication
RJ01 Rejection of invention patent application after publication

Application publication date: 20101215